US6056992A - Encapsulated additives - Google Patents

Encapsulated additives Download PDF

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US6056992A
US6056992A US08076709 US7670993A US6056992A US 6056992 A US6056992 A US 6056992A US 08076709 US08076709 US 08076709 US 7670993 A US7670993 A US 7670993A US 6056992 A US6056992 A US 6056992A
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core
food
additive
outer shell
water
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Expired - Fee Related
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US08076709
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Chel W. Lew
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Campbell Soup Co
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Campbell Soup Co
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; THEIR TREATMENT, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A23B - A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L23/00Soups; Sauces; Preparation or treatment thereof
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; THEIR TREATMENT, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A23B - A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/70Fixation, conservation, or encapsulation of flavouring agents
    • A23L27/72Encapsulation
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; THEIR TREATMENT, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A23B - A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/262Cellulose; Derivatives thereof, e.g. ethers
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; THEIR TREATMENT, NOT COVERED BY OTHER CLASSES
    • A23PSHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00Shaping or working of foodstuffs characterised by the products
    • A23P10/30Encapsulation of particles, e.g. foodstuff additives

Abstract

Edible microcapsules and a process for recovering them are disclosed. The microcapsules include a shell material that has a thermal gelation temperature within the range from about 90° F. to about 160° F. The encapsulated material is a food additive which is protected from degradation and loss during the processing at relatively high temperatures of food products. The invention is particularly useful for additives to liquid-based foods such as soups, stews, and sauces.

Description

The application is a continuation of U.S. Ser. No. 07/534,496, filed Jun. 7, 1990, now abandoned, which is a continuation-in-part of co-pending patent application U.S. Ser. No. 07/201,637, filed Jun. 2, 1988, now abandoned.

FIELD OF THE INVENTION

The invention relates to edible microcapsules containing additives, methods of making the edible microcapsules, and food products which contain them.

DESCRIPTION OF RELATED TECHNOLOGY

Food products universally contain various additives which enhance at least one characteristic of the food. Examples include volatile oils, water soluble spices, and viscosity-affecting agents. The aroma of the cooking food and the final flavor of the cooked food depend substantially on the existence and chemical form of these agents. Unfortunately, the severe processing conditions needed for the safe commercial distribution of many food products degrade or destroy many additives before the food is ultimately used by the consumer.

The problem of food additive losses is particularly acute in foods that have a water activity content of at least about 80%. Such water-based foods typically include soups, stews, and sauces. These products are usually cooked in large vats at about 140°-190° F., sealed into cans, and retorted at temperatures of at least about 250° F. for about 20 minutes to about an hour. These are exceptionally severe conditions for most food additives containing volatile oils, organic spices or both because the organic components are thermally degraded. Food additives also lose their effectiveness after only a few months of storage. The result of severe processing conditions and extended storage is a change in the flavor, aroma, odor, texture, and nutritional value of the food unless some action is taken to offset the losses.

The art has traditionally added excess levels of food additives to the food before processing to compensate for the expected losses. Alternatively, additives have been included with food products in the form of separate, discrete packages which must be mixed with the food product for consumption. High additive concentrations and separate packages, however, increase product costs and reduce the preparation convenience of the food.

Encapsulation is one method that is useful for protecting some types of additives in some foods. Encapsulated materials typically rely on a shell that is soluble in water or a shell that releases the encapsulated additive when crushed. Encapsulated materials, such as microcapsules, are to be distinguished from microspheres that exhibit a homogeneous structure and are typically formed by methods such as spray drying.

In U.S. Pat. No. 3,455,838, specific types of dextrins are used as a matrix to form a microsphere containing volatile oils for foods and cosmetics. The volatile oil is spray dried with the dextrin as an emulsion and becomes entrapped within a matrix of dextrin. The oil is released when the dextrin dissolves in water. U.S. Pat. No. 3,495,988 describes a similar process using a hydrophilic colloid (e.g., gelatin, casein, and soy protein). The bound material is blended in dry form with coffee powder and releases its active ingredient when the microspheres dissolve in water.

U.S. Pat. No. 3,712,867 describes coacervation as an encapsulation technique. One example uses a shell of acrylic acid and acrylamide. The encapsulated materials are described as including pharmaceuticals, plant protection agents, food additives, dyes, chemicals, lubricants, greases or oils, and adhesives. Due to the crosslinking possibilities with coacervates, the '867 patent suggests that it is possible to modify the water solubility of the shell so that the ingredients are released under certain conditions, e.g., upon immersion in water, under alkaline pH conditions, or with pressure (e.g., mechanical stressing or an increase in temperature).

Chewing gum is a popular product for encapsulated flavor additives. The additives are freed at body temperature by combinations of saliva, chemistry and physical crushing. U.S. Pat. Nos. 4,386,106; 4,515,769; 4,695,463; and 4,740,376 describe other encapsulated ingredients for chewing gums.

These prior encapsulation techniques, however, are not useful for water-based foods that include at least one high temperature processing step. Most encapsulating shells will not withstand the thigh processing temperatures or continue to provide protection to the additive over an extended storage period.

It would be desirable to have an encapsulated additive that could withstand food processing temperatures of at least about 200° F., protect the additive from degradation over an extended period of time at ambient storage conditions, and release the additive at an effective concentration level when the product is reheated for consumption.

SUMMARY OF THE INVENTION

It is an object of the invention to provide an encapsulated additive that enhances at least one characteristic of food product and which has a structure that protects the additive material through high processing temperatures and extended storage, but allow the additive to be released at an effective concentration when the food product is reheated for consumption.

In accordance with the object above and others that will become apparent from reading the description herein, the invention comprises an encapsulated food enhancing additive which comprises:

a core comprising: (a) at least one food enhancing additive; and (b) a meltable core material that is insoluble in water but which melts and releases said at least one additive in water at temperatures above about 90° F.; and

an outer shell completely surrounding said core, said shell comprising a shell forming material that has a thermal gelation temperature within the range from about 90° F. to about 160° F.

The invention provides a practical means for protecting a wide variety of food additives through heat processing and extended storage. The invention further reduces the quantities of food enhancing additives which must be added to a commercial food product to achieve a desired concentration when the food is consumed.

BRIEF DESCRIPTION OF THE DRAWINGS

FIGS. 1 and 2 illustrate the formation of microcapsules through stationary nozzles.

FIGS. 3 and 4 show the formation of microcapsules through submerged nozzles.

FIG. 5 is the formation of microcapsules through rotating extrusion nozzles that discharge into the air.

DETAILED DESCRIPTION OF THE INVENTION

Food enhancing additives according to the present invention can be added to virtually any comestible that is subjected to at least one high temperature processing step. Exemplary processing is heating to render the product commercially sterile. "Commercial sterility" of thermally processed food means the condition achieved by the application of heat which renders the food free of: (a) microorganisms capable of reproducing in the food under normal nonrefrigerated conditions of storage and distribution; and (b) viable microorganisms (including spores) of public health significance. Commercially sterile foods sealed in cans, jars, or pouches are beneficially affected by the present invention.

Particularly well suited are liquid-based comestibles such as sauces, stews, and soups which may contain, inter alia, vegetables, meats, and any of the many forms of pasta. Liquid-based foods are characterized by a water activity content of at least about 80% which is measured by comparing the food's vapor pressure to the vapor pressure of pure water when both liquids are at 20° C.

The term "food enhancing additive" is used broadly throughout the industry and in this application to denote any agent that affects the flavor (flavorant), aroma (odorant), viscosity, color (colorant), or nutritional value (e.g., a vitamin source) of a comestible. Examples of food additives in accordance with the invention include: food dyes, volatile and nonvolatile oils that add flavor and/or color, spices (e.g., salt and/or pepper), vitamins, and viscosity enhancing materials such as various forms of starch. The amount of food enhancing additive to be used for each type of food varies too widely to make meaningful any disclosure of a numerical range. The optimum quantity of any given additive will be determined by one in this art with no more than routine experimentation.

Canned soups are a preferred comestible for the invention, and the present invention may be conveniently described in that context. Soups are commercially prepared by the sequential steps of mixing, cooking at an elevated temperature, placing the soup into a can, sealing the can, and heating the canned food at an elevated temperature sufficient to render the soup commercially sterile. "Commercial sterility" of thermally processed food means the condition achieved by the application of heat which renders the food free of: (a) microorganisms capable of reproducing in the food under normal nonrefrigerated conditions of storage and distribution; and (b) viable microorganism (including spores) of public health significance. Suitable heat generating means include, inter alia, ovens, autoclaves, steam tunnels, and microwave chambers.

The typical cooking temperature of soup is about 140°-19° F. Suitable thermal processing includes retorting at superatmospheric conditions at temperatures of at least about 250° F. Thereafter, the food product is allowed to cool to ambient temperature, boxed, and stored at temperatures ranging from 35°-100° F. Canned soups are typically reheated to a temperature of about 140°-212° F. for consumption. The present invention uses these temperature changes and a microencapsulated food enhancing additive to provide a means by which soup additives can be added before the heat processing, protected during the relatively high treatment temperatures, and yet become available upon reheating for consumption.

Microencapsulation avoids the additive losses associated with reaction and degradation during storage. Microencapsulation also eliminates the practice of adding excess amounts of additives to compensate for storage losses.

Microcapsules according to the invention have an outer shell with a thermal gelation temperature within the range from about 90° F. (about 30° C.) to about 160° F. (about 72° C.) around a core that is microcapsule or a microsphere containing the food enhancing additive. Suitable outer shell materials include edible polymers and/or edible colloids. Particularly preferred shell materials that exhibit the desired thermal gelation temperatures are cellulose and cellulose derivative polymers such as methylcellulose, hydroxypropylcellulose, hydroxypropylmethylcellulose, and mixtures thereof. The outer shell should have a thickness sufficient to ensure coverage of the entire core surface area. Suitable thicknesses are greater than about 3μ thick, preferably about 3μ to about 50μ, and even more preferably about 10-20μ in thickness. These shell thicknesses will typically result in an outer shell weight of at least about 5 wt % of the entire microcapsule weight. The thickness and corresponding weight percentage of the shell may be increased to provide additional protection against rupture during any agitation steps that may be used in the food processing sequence.

The thermal gelation temperature of the outer shell material is the temperature at which the shell polymers start to lose their water of hydration and become insoluble in water. The start of gelation is manifested by an increase in solution viscosity and is readily determined by conventional viscosity measurements. The solution viscosity continues to increase as the solution is held at a temperature above the material gelation temperature.

Certain additives can be added to the outer shell material to affect its gelation temperature and tailor the release of the food enhancing additive to the thermal handling sequence of the food product. For example, shell additives such as sorbitol and glycerine can depress the gelation temperature by about 10° F. to about 36° F., but other shell additives such as ethanol and propylene can increase the gelation temperature by up to about 45° F. Sucrose is one shell additive that can be used to either depress or elevate the gelation temperature depending on the amount used. Adding relatively low amount, about 5 wt %, can elevate the gelation temperature up to about 10° F. yet relatively larger amounts, about 20 wt %, can depress the gelation temperature by up to about 45° F. Table 1 lists the gelation temperatures for various cellulose polymers with various shell additives.

              TABLE 1______________________________________                    Gelation          Methocel ®                    Temperature (F.)                               Methocel ®Additive   wt %   A15C      Methocel ® F15C                               K4M______________________________________none           122       145        185MgCl.sub.2   5      107       125        153Sucrose 5      124       151        183Sucrose 20     111       138        142Sorbitol   20     86        115        118Glycerine   20     93        140        149-158Ethanol 20     167       167        167Propylene   20     138       176        176______________________________________ Methocel ® A15C is a methylcellulose gum at 1500 cP viscosity Methocel ® F15C is a hydroxypropylmethylcellulose gum at 1500 cP viscosity Methocel ® K4M is a hydroxypropylmethylcellulose gum at 4000 cP viscosity

The microencapsulated additives of the invention are added to the soup when the soup is at a temperature above the outer shell gelation temperature but before the soup is thermally processed to achieve commercial sterility. The outer shell protects the food enhancing additive from the heat of the initial cooking and subsequent retortion by staying intact and not dissolving.

The gelation mechanism is, however, reversible. As the surrounding liquid cools to below the gelation temperature, the polymers become rehydrated and water soluble. For soup processing, this property means an encapsulated additive can be mixed with the soup before thermal processing and, when properly handled, can remain protected from volatilization or chemical reaction until the soup cools. Upon cooling, the outer shell dissolves and releases the food enhancing additive from the core into the soup.

The core structure should be designed to protect the food enhancing additive during the period between dissolution of the outer shell and heating the food for consumption. This storage period can, however, vary from several days to a year or more depending on the food product. Fortunately, the microcapsule core structure containing the food enhancing additive can be designed in accordance with the invention to accommodate short or extended storage periods.

The food enhancing additive is present in the core either as microsphere that is insoluble in water at the storage temperatures expected to be encountered during storage or in a core microcapsule having its own shell that is insoluble in water at the relatively cool temperatures of storage. If the core is a microsphere, the food enhancing additive is homogeneously distributed in a core matrix material that melts or otherwise dissolves when the food product is heated to an elevated temperature. Preferred core matrix materials are solid at temperatures of up to about 120° F. although the specific material chosen for use in the core should be selected so that the food enhancing additive is not released into the food before it is needed in the food cooking process.

Specific materials contemplated for use in the core include:

(1) fats that are normally solid at about 70° F., such as partially hydrogenated soybean oil, cottonseed oil, palm oil, and mixtures thereof alone or in combination with any of the mono-, di-, and triglycerides having about 14-20 carbon atoms;

(2) edible waxes, such as fully refined paraffin wax;

(3) surfactants, such as monoglycerides and lecithins; and

(4) mixtures of these materials.

The meltable microsphere core may be conveniently formed into a matrix by conventional spray drying techniques which include: (a) homogeneously mixing the core matrix material with the additive; and (b) forming droplets from the mixture. The additive and matrix may be mixed by conventional high shear mixing or emulsion forming techniques with or without emulsifiers.

The core may also be mixed with one or more materials that increases its hydrophobic properties. Exemplary hydrophobic materials include the food grade, alkaline earth stearates (e.g. calcium or magnesium stearate) and silicon dioxide in quantities of up to about 10 wt %, preferably about 4 to about 6 wt % depending on the cellulosic material used. Stearic acid may enhance precipitation if the cellulose shell has a gelation temperature between about 120° F. to about 160° F.

Another useful core structure is when the core is a microcapsule having at least one discrete shell completely surrounding a nucleus particle or core microsphere of at least one food enhancing additive. The microcapsule core shell can be made of the same material that would be used for a meltable microsphere core, i.e. hard fats, edible waxes, surfactants, and mixtures thereof. Combinations of meltable layers each containing a different food enhancing additive can be used for foods having the additives released at different times in the heating process, i.e., at different temperatures during the heating period.

The shell of a microencapsulated core is desirably greater than about 20μ in thickness, preferably about 20-35μ, and even more preferably about 20-30μin thickness. Like the outer shell, any core layers should cover the entire surface area of the underlying material to prevent premature release of the encapsulated material.

The core containing the additive in the form of a microsphere can be encapsulated with the core shell by any of the conventional mechanical or chemical techniques used to form the outer shell around the core. Preferably, successive layers are formed substantially simultaneously such as by coextrusion through annular nozzles. Linear spacing of the nozzles can be used to stagger, with small time increments, the encapsulation of the core and the encapsulation of the microcapsule core. See, FIG. 2.

The final microencapsulated food enhancing additive, regardless of core structure, may be used in a variety of sizes. The preferred sizes are within the range of about 100 to about 7,000 microns in diameter and most preferably about 900-1500 microns. The microcapsule desirably has about 30-50 wt % food enhancing additive.

As a general guideline, it is desirable to use the largest numbers of microcapsules and a reasonably low additive concentration per capsule. This practice is designed to minimize the product quality variations that might occur if a few microcapsules were not dispensed into the product due to dispensing method variations.

The microencapsulated food enhancing additives may also be made by a variety of other conventional mechanical and chemical droplet forming techniques. The preferred techniques are, however, mechanical in nature such as extrusion through stationary (FIGS. 1 and 2), submerged (FIGS. 3 and 4), or rotating extrusion nozzles (FIG. 5). Extrusion through rotating nozzles is the preferred method. Such extrusion devices are characterized by two or more concentric tubes which terminate in concentric orifices. The material from the outer nozzle(s) will surround the material from the inner nozzle(s) and form microcapsules. Additional annular tubes can be added to form additional layers as desired. Preferably, two or three concentric tubes are used to form the most preferred microcapsules of the invention. The outer shell material will pass through the outermost annular tube and surround the core microsphere or microcapsule containing the food enhancing additive.

FIG. 1 illustrates a conventional, stationary extrusion device with a central and an annular nozzle. This apparatus can be used to form a shell surrounding a microsphere core. Core material 11 containing food enhancing additive and meltable core matrix passes through central tube 12 and meets outer shell material 13 passing through outer annular tube 14. At the nozzle ends, outer shell material 13 surrounds core material 11 to form microcapsules 15. Microcapsules 15 are then collected and/or hardened by, inter alia, chemical reaction, cooling, drying, screening, centrifugation, and other equivalent techniques.

FIG. 2 illustrates a device having three extrusion tubes for encapsulating a microcapsule core containing the food enhancing additive. Microcapsule 21 exhibits outer shell 22, inner shell 23, and core 24. Core 24 may be a solid nucleus of food enhancing additive, a microsphere, or a liquid food enhancing additive. The parallel paths of the shell and core materials is similar to FIG. 1 except for the additional use of a middle annular tube 25 between outer annular tube 26 and central tube 27. Core material 28 passes through central tube 27, inner shell material 29 passes through middle annular tube 25, and outer shell material 30 passes through central tube 27.

FIG. 3 depicts a submerged extrusion nozzle. The depicted nozzle has three tubes like FIG. 2, but outer shell material 31 is passed through middle tube 32 and core material 33 is passed through central tube 34. Carrier fluid 35 moves through outer tube 38 at a sufficient flowrate to carry microcapsules 36 to the hardening zone 37. Carrier fluid 35 conveniently contains any chemical reactants, hardening agents, or immiscible liquids that will cause microcapsules 36 to form and/or harden quickly. Heating medium 39 flows through hardening zone 37 to cause outer shell material 31 to harden around core material 33.

Preferred carrier fluids 35 contain common salt (NaCl) in concentration of at least about 10 wt %, preferably at least about 12 wt %, and most preferably at least about 15 wt % salt based on the total weight. Salt is particularly useful for producing a hard microcapsule when using outer shell materials that are sensitive to salt.

Salt solutions are a desirable medium in which to form the microcapsules because it has been determined that the resulting microcapsules do not become tacky or have a tendency to clump together after they are removed from the formation solution. Such a medium is also compatible with a microcapsule which comprises an inner material of fat and salt around which is formed the encapsulating outer shell. The high temperature relatively for the concentrated salt solution ensures that the encapsulating shell will not dissolve in water.

FIG. 4 depicts a submerged extrusion system where the three tube extruder of FIG. 2 is modified to encapsulate microcapsule cores. Core material 413 passes through central tube 414. Core shell material 415 passes through first annular tube 416. Outer shell material 417 passes through second annular tube 418. The revised extruder includes a fourth annular tube 411 for carrier fluid 412. Carrier fluid 412 can include hardening additives as described above. Additional carrier fluid 419 is pumped into transport zone 420 for passage to recovery zone 421 which comprises screen 422 over tank 423.

Heater/chiller units 424 are used to control the temperature of carrier fluid 412 and 419. Carrier fluids 412 and 419 are desirably maintained at a temperature above the thermal gelation temperature of the outer shell material, e.g. above about 90° F. As with the embodiment of FIG. 3, carrier fluids 412 and 419 can contain appropriate salts (e.g., sodium chloride) in amounts sufficient to encourage the outer shell to harden.

FIG. 5 illustrates a set of rotating extrusion nozzles 51 that rotate on a horizontal plane at a rate of about 100 to several thousand rpm and form encapsulated microspheres. The basic construction details are similar to stationary nozzle 1 in that core material 52 is passed through the central tube 53 while outer shell material 54 passes through annular tube 55. Central tube 53 and annular tube 55, however, bend at an angle α of about 60-120° from vertical, preferably about 90°, to produce a centrifugal force on the microcapsule materials. The degree of that force and the size of the resulting microcapsule can be controlled by adjusting the rotation rate of drive shaft 56. For example, a core of an edible fat and a shell of a cellulosic material will form microcapsules having a diameter of about 1 mm with an orifice size of about 0.020-0.040 inches and a rotation rate of about 500 rpm.

The extruded microspheres from rotating nozzles 51 are desirably released from the extruder into free fall for sphere formation and then collected in a salt-containing bath. The bath preferably contains at least about 10 wt %, preferably at least about 12 wt %, and most preferably about 15 wt % salt based on the total weight. Like the submerged system above, salt is particularly useful for producing a hard microcapsule when using outer shell materials that are sensitive to salt.

Surfactants may be used in the salt collection bath to reduce the interfacial tension of the bath and the flattening forces encountered upon impact of the particle with the liquid surface. Appropriate concentrations are readily determinable with no more than routine tests.

Other chemical microcapsule manufacturing techniques that can be used to form microencapsulated food enhancing additives according to the invention include coacervation and phase separation. A description of these techniques can be found in U.S. Pat. Nos. 3,712,867 (coacervation) and 4,211,668 (emulsion) which are herein incorporated by reference.

The present invention is conveniently described with reference to the following examples.

EXAMPLES

Flavoring agents containing a small amount of trans-2-hexanal and hexanal as tracer material were formed into a microsphere with a partially hydrogenated vegetable oil as a hard fat. The microsphere core was then encapsulated in a cellulosic shell by extrusion through rotating nozzles. The microcapsules were sized to be no larger than 1 mm in diameter and collected in a 15% salt solution. The salt solution was at a temperature of 170°-180° F.

The microencapsulated additives were added to soup when the soup had a temperature of about 160° F. The soup containing the microencapsulated additive were then heated in a retort at about 250° F. for 30-60 minutes to achieve commercial sterility.

______________________________________     Shell Composition                     Fill CompositionExample   (wt %, dry basis)                     (wt %)______________________________________1         83% Methocel ® E-3                     100% flavor mix in     17% sorbitol    cottonseed oil2         99.9% Methocel ® E-3                     70% Durkee ® KLX     0.1% Tandem ® 552                     30% flavor mix3         83% Methocel ® E-3                     70% Durkee ® KLX     17% sorbitol    30% flavor mix     0.1% Tandem ® 552______________________________________ *Durkee KLX is a partially hydrogenated vegetable oil *Methocel ® E3 is a hydroxypropylmethylcellulose. *Tandem ® 552 is a food grade emulsifier blend of mono and diglycerides, polysorbate 60, water, BHA, and citric acid.

The soup was measured weekly for two months and biweekly for four months thereafter for the release of trans-2-hexanal and hexanal. The presence of these agents indicates the release of the encapsulated materials and breakdown of the core structure. The encapsulated flavoring agents showed good stability and resistance to degradation over extended storage periods of 50 days.

The examples are set forth for purposes of illustration only and are not intended to be construed as limitations on the scope of the appended claims.

Claims (9)

What is claimed is:
1. A method for making edible microcapsules, said method comprising:
forming an edible microcapsule having:
a) a core comprising: (i) at least one food enhancing additive; and (ii) a meltable core material that is insoluble in water but which melts and releases said at least one additive in water at temperatures above about 90° F.; and
b) an outer shell completely surrounding said core, said outer shell comprising a shell forming material that has a thermal gelation temperature within the range from about 90° F. to about 160° F.;
collecting the microcapsule in an aqueous solution at a temperature greater than about 140° F. containing at least about 10 wt % sodium chloride.
2. The method according to claim 1 wherein said aqueous solution comprises at least about 12 wt % sodium chloride.
3. The method according to claim 2 wherein said aqueous solution comprises at least about 15 wt % sodium chloride.
4. The method according to claim 2 wherein the forming step comprises surrounding said food additive with a shell material selected from the group consisting of hydroxymethylcellulose and methylcellulose.
5. A method according to claim 1 wherein said at least one food enhancing additive comprises a spice.
6. A method according to claim 5 wherein said at least one food enhancing additive comprises a spice.
7. A process for preparing a liquid-based food product, said process comprising:
adding to a liquid-based food product a microencapsulated food enhancing additive comprising:
a) a core comprising: (i) at least one food enhancing additive; and (ii) a meltable core material that is insoluble in water but which melts and releases said at least one additive in water at temperatures above about 90° F.; and
b) an outer shell completely surrounding said core, said outer shell comprising a shell forming material that has a thermal gelation temperature within the range from about 90° F. to about 160° F.; and
heating said food product containing said additive at an elevated temperature for a time sufficient to render said food product commercially sterile; and
allowing the commercially sterile food product to cool so said outer shell dissolves and releases said core into the food product.
8. The process according to claim 7 further comprising:
heating the food product containing the released core at an elevated temperature and for a time sufficient to release said food enhancing additive from said core.
9. A method for making edible microcapsules, said method comprising:
forming an edible microcapsule having:
a) a core comprising: (i) at least one food enhancing additive; and (ii) a meltable core material that is insoluble in water but which melts and releases said at least one additive in water at temperatures above about 90° F.; and
b) an outer shell completely surrounding said core, said outer shell comprising methylcellulose.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020187221A1 (en) * 2001-04-26 2002-12-12 Takasago International Corporation Coating agent and coated powder
US20030124228A1 (en) * 2001-04-26 2003-07-03 Takasago International Corporation Coating agent and coated powder
US6610348B2 (en) 1997-02-17 2003-08-26 Fonterra Tech Limited Gelling agents and gels containing them
US20040156953A1 (en) * 2003-02-12 2004-08-12 Guidry Ray A. Encapsulated food additives and method for preparing foodstuffs
WO2004089113A1 (en) * 2003-04-08 2004-10-21 Quest International B.V. Oxigen stable active containing compositions
US20050260266A1 (en) * 2003-11-21 2005-11-24 Cadbury Adams Usa, Llc. Controlled release oral delivery systems
US20060024245A1 (en) * 2004-07-29 2006-02-02 Cadbury Adams, Llc. Tooth whitening compositions and delivery systems therefor
US7041277B2 (en) * 2000-03-10 2006-05-09 Cadbury Adams Usa Llc Chewing gum and confectionery compositions with encapsulated stain removing agent compositions, and methods of making and using the same
US20060124695A1 (en) * 2003-06-27 2006-06-15 Wakunaga Pharmaceutical Co., Ltd. Stable liquid preparation
US20070053972A1 (en) * 2005-09-08 2007-03-08 Cadbury Adams Usa Llc. Gelatin capsules containing actives
US20070059407A1 (en) * 2005-09-09 2007-03-15 Donald Spector Flavor shakers with encapsulation
US20070071808A1 (en) * 2003-08-28 2007-03-29 Janik John J Capsule filled with honey
US20080029110A1 (en) * 2006-02-10 2008-02-07 R. J. Reynolds Tobacco Company Smokeless Tobacco Composition
US20080075813A1 (en) * 2006-09-27 2008-03-27 Gordon Smith Seasoning and method for enhancing and potentiating food flavor utilizing microencapsulation while reducing dietary sodium intake
US20080317681A1 (en) * 2003-07-11 2008-12-25 Petros Gebreselassie Compositions containing a stain removing complex, and methods of making and using the same
EP2179666A2 (en) 2007-07-23 2010-04-28 R.J.Reynolds Tobacco Company Smokeless Tobacco Compositions And Methods For Treating Tobacco For Use Therein
US7727565B2 (en) 2004-08-25 2010-06-01 Cadbury Adams Usa Llc Liquid-filled chewing gum composition
WO2010063937A1 (en) 2008-12-01 2010-06-10 Capsum Method for manufacturing capsule series, and related capsule series
US20100297303A1 (en) * 2009-05-20 2010-11-25 Conopco, Inc., D/B/A Unilever Unitized frozen sauce products
US7851000B2 (en) 2005-05-23 2010-12-14 Cadbury Adams Usa Llc Taste potentiator compositions and edible confectionery and chewing gum products containing same
US7851005B2 (en) 2005-05-23 2010-12-14 Cadbury Adams Usa Llc Taste potentiator compositions and beverages containing same
US7851006B2 (en) 2005-05-23 2010-12-14 Cadbury Adams Usa Llc Taste potentiator compositions and beverages containing same
US20110097449A1 (en) * 2006-06-30 2011-04-28 Conagra Foods Rdm, Inc. Seasoning and method for seasoning a food product while reducing dietary sodium intake
US7955630B2 (en) 2004-09-30 2011-06-07 Kraft Foods Global Brands Llc Thermally stable, high tensile strength encapsulated actives
WO2011086331A2 (en) 2010-01-15 2011-07-21 Capsum Method for manufacturing capsules having controlled head
WO2011140430A1 (en) 2010-05-07 2011-11-10 R. J. Reynolds Tobacco Company Filtered cigarette with modifiable sensory characteristics
WO2012103327A1 (en) 2011-01-28 2012-08-02 R. J. Reynolds Tobacco Company Polymeric materials derived from tobacco
US8389031B2 (en) 2005-05-23 2013-03-05 Kraft Foods Global Brands Llc Coated delivery system for active components as part of an edible composition
US8389032B2 (en) 2005-05-23 2013-03-05 Kraft Foods Global Brands Llc Delivery system for active components as part of an edible composition having selected particle size
US8591973B2 (en) 2005-05-23 2013-11-26 Kraft Foods Global Brands Llc Delivery system for active components and a material having preselected hydrophobicity as part of an edible composition
US8591968B2 (en) 2005-05-23 2013-11-26 Kraft Foods Global Brands Llc Edible composition including a delivery system for active components
US8591972B2 (en) 2005-05-23 2013-11-26 Kraft Foods Global Brands Llc Delivery system for coated active components as part of an edible composition
US8591974B2 (en) 2003-11-21 2013-11-26 Kraft Foods Global Brands Llc Delivery system for two or more active components as part of an edible composition
US8597703B2 (en) 2005-05-23 2013-12-03 Kraft Foods Global Brands Llc Delivery system for active components as part of an edible composition including a ratio of encapsulating material and active component
CN103635252A (en) * 2011-03-08 2014-03-12 卡普苏姆公司 Method for forming drops of a first phase dispersed in a second phase substantially immiscible with the first phase
US8828423B2 (en) 2003-11-21 2014-09-09 Intercontinental Great Brands Llc Delivery system for active components as part of an edible composition having preselected tensile strength
US9011946B2 (en) 2011-04-29 2015-04-21 Intercontinental Great Brands Llc Encapsulated acid, method for the preparation thereof, and chewing gum comprising same
US9198448B2 (en) 2005-02-07 2015-12-01 Intercontinental Great Brands Llc Stable tooth whitening gum with reactive ingredients
WO2016090075A1 (en) 2014-12-05 2016-06-09 R. J. Reynolds Tobacco Company Smokeless tobacco pouch
WO2017093941A1 (en) 2015-12-03 2017-06-08 Niconovum Usa, Inc. Multi-phase delivery compositions and products incorporating such compositions

Citations (104)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA968248A1 (en)
US1264592A (en) * 1917-05-21 1918-04-30 Frederick C Atkinson Baking-powder and process of making same.
US1286904A (en) * 1917-05-21 1918-12-10 Frederick C Atkinson Baking-powder and process of making same.
US2183173A (en) * 1938-12-22 1939-12-12 Jefferson Island Salt Mining C Method of treating salt and resulting product
US2539012A (en) * 1948-08-11 1951-01-23 Gen Foods Corp Salt product
US2560830A (en) * 1945-10-22 1951-07-17 American Dairies Inc Feed for ruminant animals
US2799241A (en) * 1949-01-21 1957-07-16 Wisconsin Alumni Res Found Means for applying coatings to tablets or the like
US2819971A (en) * 1955-10-06 1958-01-14 Gen Foods Corp Food product and process
US2921883A (en) * 1957-05-03 1960-01-19 Smith Kline French Lab Novel coating material for medicaments
US2956926A (en) * 1958-09-23 1960-10-18 American Cyanamid Co Coated citric acid particles
US2970911A (en) * 1958-03-19 1961-02-07 Hoffman Taff Inc Choline-fat composition
US3009810A (en) * 1959-01-07 1961-11-21 Gen Foods Corp Fumaric acid composition
US3015128A (en) * 1960-08-18 1962-01-02 Southwest Res Inst Encapsulating apparatus
US3082154A (en) * 1960-04-19 1963-03-19 Ici Ltd Improved free-flowing coated antimalarial salts in particulate form
GB936386A (en) 1959-01-16 1963-09-11 Wellcome Found Pellets for supplying biologically active substances to ruminants
US3110626A (en) * 1961-08-17 1963-11-12 Minnesota Mining & Mfg Apparatus for coating discrete solid material
US3131068A (en) * 1961-07-24 1964-04-28 American Cyanamid Co Water-soluble coated edible organic acids
US3147187A (en) * 1962-09-10 1964-09-01 Don Hall Lab Sustained release pharmaceutical
GB972128A (en) 1960-01-21 1964-10-07 Wellcome Found Pellets for supplying biologically active substances to ruminants and the manufacture of such pellets
US3159874A (en) * 1962-08-02 1964-12-08 Iit Res Inst Apparatus for electrostatic encapsulation
US3279994A (en) * 1963-02-19 1966-10-18 Hoffmann La Roche Riboflavin beadlet composition
US3334584A (en) * 1962-09-24 1967-08-08 William C Toland Production of lithographic printing plates
US3336155A (en) * 1964-01-15 1967-08-15 Ncr Co Process of coating particles with a polymer
US3341466A (en) * 1966-10-31 1967-09-12 Brynko Carl Process for making capsules
US3455838A (en) * 1966-04-22 1969-07-15 Nat Starch Chem Corp Method of encapsulating water-insoluble substances and product thereof
US3471304A (en) * 1966-03-07 1969-10-07 Archer Daniels Midland Co Edible coating compositions
US3475177A (en) * 1966-02-09 1969-10-28 Commercial Solvents Corp Choline composition
US3495988A (en) * 1968-03-06 1970-02-17 Leslie L Balassa Encapsulation of aromas and flavors
US3523906A (en) * 1962-07-11 1970-08-11 Gevaert Photo Prod Nv Process for encapsulating water and compounds in aqueous phase by evaporation
US3541204A (en) * 1968-12-02 1970-11-17 Ian Ramsay Sibbald Encapsulated biologically active materials for feeding to ruminants and process for the production thereof
US3641236A (en) * 1968-07-16 1972-02-08 Delandale Lab Ltd Dosage unit sustained release oral powdered lithium salt composition for manic depressive or depressive illness prophylactic therapy
US3663271A (en) * 1969-03-26 1972-05-16 Organon Surface-modified acid crystals and process for their preparation
US3712867A (en) * 1970-03-04 1973-01-23 Bayer Ag Process for the production of microcapsules with the aid of synthetic coacervates and microcapsules produced thereby
US3726805A (en) * 1970-03-17 1973-04-10 Fuji Photo Film Co Ltd Process for the production of amino acid-containing microcapsules
US3743512A (en) * 1970-09-16 1973-07-03 F Hansen Monoglyceride product and method of preparing the same
US3767421A (en) * 1971-01-19 1973-10-23 Gen Mills Inc Shelf stable, intermediate moisture doughs
US3819838A (en) * 1970-08-04 1974-06-25 Bush Boake Allen Ltd Encapsulated flavoring composition
US3856699A (en) * 1969-08-08 1974-12-24 Fuji Photo Film Co Ltd Process for producing capsules having walls of a waxy material
US3867556A (en) * 1972-12-21 1975-02-18 Procter & Gamble Fats with encapsulated flavors
US3876809A (en) * 1973-06-08 1975-04-08 Int Flavors & Fragrances Inc Dialkyl dihydroxy dithianes as flavoring agents
US3906116A (en) * 1972-09-25 1975-09-16 Bush Boake Allen Ltd Concentrated oleoresin products and emulsification process for preparing them
US3922379A (en) * 1973-12-17 1975-11-25 Abbott Lab Microencapsulation process
US3959493A (en) * 1971-03-17 1976-05-25 Rumen Chemie, Ag Rumen bypass products comprising biologically active substances protected with aliphatic fatty acids
US3959499A (en) * 1974-12-23 1976-05-25 The United States Of America As Represented By The Secretary Of The Army Leavening composition and storage stable cake mixes made therewith
US3962416A (en) * 1971-01-25 1976-06-08 Sol Katzen Preserved nutrients and products
US3965033A (en) * 1970-07-27 1976-06-22 Fuji Photo Film Co., Ltd. Process for the production of oil-containing microcapsules
US3975280A (en) * 1974-03-21 1976-08-17 Henkel & Cie G.M.B.H. Storage-stable, readily-soluble detergent additives, coating compositions and process
US3985913A (en) * 1974-07-31 1976-10-12 Scm Corporation Condiment encapsulation by spray drying
US4001480A (en) * 1974-08-16 1977-01-04 Swift & Company Encapsulation process utilizing microorganisms and products produced thereby
US4045587A (en) * 1970-01-13 1977-08-30 International Flavors & Fragrances Inc. Foodstuff flavoring methods and compositions
US4123382A (en) * 1973-05-25 1978-10-31 Merck & Co., Inc. Method of microencapsulation
US4141998A (en) * 1975-12-31 1979-02-27 William H. Ziemke Baking ingredient for sourdough compositions
US4196187A (en) * 1977-09-02 1980-04-01 Eastman Kodak Company Rumen-stable pellets
US4211668A (en) * 1977-03-07 1980-07-08 Thalatta, Inc. Process of microencapsulation and products thereof
US4217370A (en) * 1977-08-25 1980-08-12 Blue Wing Corporation Lipid-containing feed supplements and foodstuffs
US4232047A (en) * 1978-05-30 1980-11-04 Griffith Laboratories U.S.A., Inc. Food supplement concentrate in a dense glasseous extrudate
US4259355A (en) * 1979-03-05 1981-03-31 International Flavors & Fragrances Inc. Chewing gum containing flavor composition and flavor composition therefor
US4267198A (en) * 1978-06-27 1981-05-12 Daicel Ltd. Melt-coated preparation containing sorbic acid
US4276312A (en) * 1978-05-25 1981-06-30 Merritt Carleton G Encapsulation of materials
US4288460A (en) * 1979-05-24 1981-09-08 Balchem Corporation Non-caking, water-soluble, granular coated food ingredient
US4333919A (en) * 1979-09-12 1982-06-08 Eli Lilly And Company Growth promotant controlled release formulations and method of treatment
US4351825A (en) * 1979-02-02 1982-09-28 Orion-Yhtyma Oy Process for the preparation of tablets with retarded liberation of the active agent is predetermined
US4384975A (en) * 1980-06-13 1983-05-24 Sandoz, Inc. Process for preparation of microspheres
US4386106A (en) * 1981-12-01 1983-05-31 Borden, Inc. Process for preparing a time delayed release flavorant and an improved flavored chewing gum composition
US4409257A (en) * 1982-05-25 1983-10-11 Mccormick & Company, Inc. Homogeneous, free-flowing liquid black pepper oleoresin composition
US4460563A (en) * 1980-04-09 1984-07-17 Eurand S.P.A. Process for preparing microcapsules in a liquid vehicle
US4497845A (en) * 1982-03-11 1985-02-05 Scm Corporation Acidulated meat emulsion
US4511584A (en) * 1983-05-31 1985-04-16 Scm Corporation Particulate food acidulant
US4515769A (en) * 1981-12-01 1985-05-07 Borden, Inc. Encapsulated flavorant material, method for its preparation, and food and other compositions incorporating same
US4537784A (en) * 1983-05-31 1985-08-27 Scm Corporation Process of preparing a particulate food acidulant
US4563212A (en) * 1983-12-27 1986-01-07 Monsanto Company High concentration encapsulation by interfacial polycondensation
US4595584A (en) * 1983-05-26 1986-06-17 Eastman Kodak Company Rumen-stable pellets
US4606940A (en) * 1984-12-21 1986-08-19 The Ohio State University Research Foundation Small particle formation and encapsulation
US4608277A (en) * 1983-09-17 1986-08-26 Casella Aktiengesellschaft Encapsulated salts of sparing solubility in water, their preparation and their use
US4640709A (en) * 1984-06-12 1987-02-03 Monsanto Company High concentration encapsulation by interfacial polycondensation
US4671963A (en) * 1983-10-28 1987-06-09 Germino Felix J Stearate treated food products
US4673595A (en) * 1984-10-17 1987-06-16 Debiopharm, S.A. Microencapsulation by phase separation of water-soluble medicaments
US4687676A (en) * 1982-07-12 1987-08-18 Eastman Kodak Company Rumen-stable pellets
US4695467A (en) * 1984-07-12 1987-09-22 Fujisawa Pharmaceutical Co., Ltd. Sustained release tablet
US4695463A (en) * 1985-05-24 1987-09-22 Warner-Lambert Company Delivery system for active ingredients and preparation thereof
US4713245A (en) * 1984-06-04 1987-12-15 Mitsui Toatsu Chemicals, Incorporated Granule containing physiologically-active substance, method for preparing same and use thereof
US4717567A (en) * 1985-11-25 1988-01-05 Eastman Kodak Company Rumen-stable pellets
US4740376A (en) * 1986-01-07 1988-04-26 Warner-Lambert Company Encapsulation composition for use with chewing gum and edible products
US4749575A (en) * 1983-10-03 1988-06-07 Bio-Dar Ltd. Microencapsulated medicament in sweet matrix
US4764317A (en) * 1984-02-09 1988-08-16 Southwest Research Institute Microencapsulation process and apparatus
US4772477A (en) * 1986-10-17 1988-09-20 Balchem Corporation Meat acidulant
US4797288A (en) * 1984-10-05 1989-01-10 Warner-Lambert Company Novel drug delivery system
US4832967A (en) * 1986-11-17 1989-05-23 Rhone-Poulenc Sante Composition for feeding ruminants containing a biologically active substance and its preparation
US4837004A (en) * 1985-10-18 1989-06-06 Eastman Kodak Company Rumen-stable pellets
US4842863A (en) * 1987-01-26 1989-06-27 Showa Denko Kabushiki Kaisha Granular agent for ruminant and production method thereof
US4876097A (en) * 1984-12-20 1989-10-24 Rhone-Poulenc Sante Compositions for coating feeding stuff additives intended for ruminants and feeding stuff additives thus coated
US4880646A (en) * 1988-11-29 1989-11-14 Southwest Research Institute Encapsulated corn kernels and method of forming the same
US4971804A (en) * 1989-02-02 1990-11-20 Warner-Lambert Company Water dispersible gemfibrozil compositions
US4990341A (en) * 1986-10-31 1991-02-05 Euroceltique, S.A. Controlled release hydromorphone composition
US5043169A (en) * 1990-05-25 1991-08-27 Warner-Lambert Company Stabilized Sweetner Composition
US5064650A (en) * 1988-04-19 1991-11-12 Southwest Research Institute Controlled-release salt sensitive capsule for oral use and adhesive system
US5093128A (en) * 1989-07-18 1992-03-03 Draguesku Oliver J Rumen and other stomach chamber bypass nutrients and methods of fabrication
US5132125A (en) * 1988-11-29 1992-07-21 Southwest Research Institute Encapsulated corn kernels and method of forming the same
US5164195A (en) * 1988-04-19 1992-11-17 Southwest Research Institute Method of oral delivery with an adherent controlled-release salt sensitive capsule
US5167962A (en) * 1990-05-23 1992-12-01 Southwest Research Institute Filament system for delivering a medicament and method
US5167947A (en) * 1989-10-26 1992-12-01 Southwest Research Institute Enhancement of absorption of radioprotective drugs
US5190775A (en) * 1991-05-29 1993-03-02 Balchem Corporation Encapsulated bioactive substances
US5246636A (en) * 1991-05-07 1993-09-21 Southwest Research Institute Process for making microcapsules and apparatus therefor
US5254598A (en) 1991-12-09 1993-10-19 Southwest Research Institute Biodegradable composition and products

Patent Citations (104)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA968248A1 (en)
US1264592A (en) * 1917-05-21 1918-04-30 Frederick C Atkinson Baking-powder and process of making same.
US1286904A (en) * 1917-05-21 1918-12-10 Frederick C Atkinson Baking-powder and process of making same.
US2183173A (en) * 1938-12-22 1939-12-12 Jefferson Island Salt Mining C Method of treating salt and resulting product
US2560830A (en) * 1945-10-22 1951-07-17 American Dairies Inc Feed for ruminant animals
US2539012A (en) * 1948-08-11 1951-01-23 Gen Foods Corp Salt product
US2799241A (en) * 1949-01-21 1957-07-16 Wisconsin Alumni Res Found Means for applying coatings to tablets or the like
US2819971A (en) * 1955-10-06 1958-01-14 Gen Foods Corp Food product and process
US2921883A (en) * 1957-05-03 1960-01-19 Smith Kline French Lab Novel coating material for medicaments
US2970911A (en) * 1958-03-19 1961-02-07 Hoffman Taff Inc Choline-fat composition
US2956926A (en) * 1958-09-23 1960-10-18 American Cyanamid Co Coated citric acid particles
US3009810A (en) * 1959-01-07 1961-11-21 Gen Foods Corp Fumaric acid composition
GB936386A (en) 1959-01-16 1963-09-11 Wellcome Found Pellets for supplying biologically active substances to ruminants
GB972128A (en) 1960-01-21 1964-10-07 Wellcome Found Pellets for supplying biologically active substances to ruminants and the manufacture of such pellets
US3082154A (en) * 1960-04-19 1963-03-19 Ici Ltd Improved free-flowing coated antimalarial salts in particulate form
US3015128A (en) * 1960-08-18 1962-01-02 Southwest Res Inst Encapsulating apparatus
US3131068A (en) * 1961-07-24 1964-04-28 American Cyanamid Co Water-soluble coated edible organic acids
US3110626A (en) * 1961-08-17 1963-11-12 Minnesota Mining & Mfg Apparatus for coating discrete solid material
US3523906A (en) * 1962-07-11 1970-08-11 Gevaert Photo Prod Nv Process for encapsulating water and compounds in aqueous phase by evaporation
US3159874A (en) * 1962-08-02 1964-12-08 Iit Res Inst Apparatus for electrostatic encapsulation
US3147187A (en) * 1962-09-10 1964-09-01 Don Hall Lab Sustained release pharmaceutical
US3334584A (en) * 1962-09-24 1967-08-08 William C Toland Production of lithographic printing plates
US3279994A (en) * 1963-02-19 1966-10-18 Hoffmann La Roche Riboflavin beadlet composition
US3336155A (en) * 1964-01-15 1967-08-15 Ncr Co Process of coating particles with a polymer
US3475177A (en) * 1966-02-09 1969-10-28 Commercial Solvents Corp Choline composition
US3471304A (en) * 1966-03-07 1969-10-07 Archer Daniels Midland Co Edible coating compositions
US3455838A (en) * 1966-04-22 1969-07-15 Nat Starch Chem Corp Method of encapsulating water-insoluble substances and product thereof
US3341466A (en) * 1966-10-31 1967-09-12 Brynko Carl Process for making capsules
US3495988A (en) * 1968-03-06 1970-02-17 Leslie L Balassa Encapsulation of aromas and flavors
US3641236A (en) * 1968-07-16 1972-02-08 Delandale Lab Ltd Dosage unit sustained release oral powdered lithium salt composition for manic depressive or depressive illness prophylactic therapy
US3541204A (en) * 1968-12-02 1970-11-17 Ian Ramsay Sibbald Encapsulated biologically active materials for feeding to ruminants and process for the production thereof
US3663271A (en) * 1969-03-26 1972-05-16 Organon Surface-modified acid crystals and process for their preparation
US3856699A (en) * 1969-08-08 1974-12-24 Fuji Photo Film Co Ltd Process for producing capsules having walls of a waxy material
US4045587A (en) * 1970-01-13 1977-08-30 International Flavors & Fragrances Inc. Foodstuff flavoring methods and compositions
US3712867A (en) * 1970-03-04 1973-01-23 Bayer Ag Process for the production of microcapsules with the aid of synthetic coacervates and microcapsules produced thereby
US3726805A (en) * 1970-03-17 1973-04-10 Fuji Photo Film Co Ltd Process for the production of amino acid-containing microcapsules
US3965033A (en) * 1970-07-27 1976-06-22 Fuji Photo Film Co., Ltd. Process for the production of oil-containing microcapsules
US3819838A (en) * 1970-08-04 1974-06-25 Bush Boake Allen Ltd Encapsulated flavoring composition
US3743512A (en) * 1970-09-16 1973-07-03 F Hansen Monoglyceride product and method of preparing the same
US3767421A (en) * 1971-01-19 1973-10-23 Gen Mills Inc Shelf stable, intermediate moisture doughs
US3962416A (en) * 1971-01-25 1976-06-08 Sol Katzen Preserved nutrients and products
US3959493A (en) * 1971-03-17 1976-05-25 Rumen Chemie, Ag Rumen bypass products comprising biologically active substances protected with aliphatic fatty acids
US3906116A (en) * 1972-09-25 1975-09-16 Bush Boake Allen Ltd Concentrated oleoresin products and emulsification process for preparing them
US3867556A (en) * 1972-12-21 1975-02-18 Procter & Gamble Fats with encapsulated flavors
US4123382A (en) * 1973-05-25 1978-10-31 Merck & Co., Inc. Method of microencapsulation
US3876809A (en) * 1973-06-08 1975-04-08 Int Flavors & Fragrances Inc Dialkyl dihydroxy dithianes as flavoring agents
US3922379A (en) * 1973-12-17 1975-11-25 Abbott Lab Microencapsulation process
US3975280A (en) * 1974-03-21 1976-08-17 Henkel & Cie G.M.B.H. Storage-stable, readily-soluble detergent additives, coating compositions and process
US3985913A (en) * 1974-07-31 1976-10-12 Scm Corporation Condiment encapsulation by spray drying
US4001480A (en) * 1974-08-16 1977-01-04 Swift & Company Encapsulation process utilizing microorganisms and products produced thereby
US3959499A (en) * 1974-12-23 1976-05-25 The United States Of America As Represented By The Secretary Of The Army Leavening composition and storage stable cake mixes made therewith
US4141998A (en) * 1975-12-31 1979-02-27 William H. Ziemke Baking ingredient for sourdough compositions
US4211668A (en) * 1977-03-07 1980-07-08 Thalatta, Inc. Process of microencapsulation and products thereof
US4217370A (en) * 1977-08-25 1980-08-12 Blue Wing Corporation Lipid-containing feed supplements and foodstuffs
US4196187A (en) * 1977-09-02 1980-04-01 Eastman Kodak Company Rumen-stable pellets
US4276312A (en) * 1978-05-25 1981-06-30 Merritt Carleton G Encapsulation of materials
US4232047A (en) * 1978-05-30 1980-11-04 Griffith Laboratories U.S.A., Inc. Food supplement concentrate in a dense glasseous extrudate
US4267198A (en) * 1978-06-27 1981-05-12 Daicel Ltd. Melt-coated preparation containing sorbic acid
US4351825A (en) * 1979-02-02 1982-09-28 Orion-Yhtyma Oy Process for the preparation of tablets with retarded liberation of the active agent is predetermined
US4259355A (en) * 1979-03-05 1981-03-31 International Flavors & Fragrances Inc. Chewing gum containing flavor composition and flavor composition therefor
US4288460A (en) * 1979-05-24 1981-09-08 Balchem Corporation Non-caking, water-soluble, granular coated food ingredient
US4333919A (en) * 1979-09-12 1982-06-08 Eli Lilly And Company Growth promotant controlled release formulations and method of treatment
US4460563A (en) * 1980-04-09 1984-07-17 Eurand S.P.A. Process for preparing microcapsules in a liquid vehicle
US4384975A (en) * 1980-06-13 1983-05-24 Sandoz, Inc. Process for preparation of microspheres
US4515769A (en) * 1981-12-01 1985-05-07 Borden, Inc. Encapsulated flavorant material, method for its preparation, and food and other compositions incorporating same
US4386106A (en) * 1981-12-01 1983-05-31 Borden, Inc. Process for preparing a time delayed release flavorant and an improved flavored chewing gum composition
US4497845A (en) * 1982-03-11 1985-02-05 Scm Corporation Acidulated meat emulsion
US4409257A (en) * 1982-05-25 1983-10-11 Mccormick & Company, Inc. Homogeneous, free-flowing liquid black pepper oleoresin composition
US4687676A (en) * 1982-07-12 1987-08-18 Eastman Kodak Company Rumen-stable pellets
US4595584A (en) * 1983-05-26 1986-06-17 Eastman Kodak Company Rumen-stable pellets
US4511584A (en) * 1983-05-31 1985-04-16 Scm Corporation Particulate food acidulant
US4537784A (en) * 1983-05-31 1985-08-27 Scm Corporation Process of preparing a particulate food acidulant
US4608277A (en) * 1983-09-17 1986-08-26 Casella Aktiengesellschaft Encapsulated salts of sparing solubility in water, their preparation and their use
US4749575A (en) * 1983-10-03 1988-06-07 Bio-Dar Ltd. Microencapsulated medicament in sweet matrix
US4671963A (en) * 1983-10-28 1987-06-09 Germino Felix J Stearate treated food products
US4563212A (en) * 1983-12-27 1986-01-07 Monsanto Company High concentration encapsulation by interfacial polycondensation
US4764317A (en) * 1984-02-09 1988-08-16 Southwest Research Institute Microencapsulation process and apparatus
US4713245A (en) * 1984-06-04 1987-12-15 Mitsui Toatsu Chemicals, Incorporated Granule containing physiologically-active substance, method for preparing same and use thereof
US4640709A (en) * 1984-06-12 1987-02-03 Monsanto Company High concentration encapsulation by interfacial polycondensation
US4695467A (en) * 1984-07-12 1987-09-22 Fujisawa Pharmaceutical Co., Ltd. Sustained release tablet
US4797288A (en) * 1984-10-05 1989-01-10 Warner-Lambert Company Novel drug delivery system
US4673595A (en) * 1984-10-17 1987-06-16 Debiopharm, S.A. Microencapsulation by phase separation of water-soluble medicaments
US4876097A (en) * 1984-12-20 1989-10-24 Rhone-Poulenc Sante Compositions for coating feeding stuff additives intended for ruminants and feeding stuff additives thus coated
US4606940A (en) * 1984-12-21 1986-08-19 The Ohio State University Research Foundation Small particle formation and encapsulation
US4695463A (en) * 1985-05-24 1987-09-22 Warner-Lambert Company Delivery system for active ingredients and preparation thereof
US4837004A (en) * 1985-10-18 1989-06-06 Eastman Kodak Company Rumen-stable pellets
US4717567A (en) * 1985-11-25 1988-01-05 Eastman Kodak Company Rumen-stable pellets
US4740376A (en) * 1986-01-07 1988-04-26 Warner-Lambert Company Encapsulation composition for use with chewing gum and edible products
US4772477A (en) * 1986-10-17 1988-09-20 Balchem Corporation Meat acidulant
US4990341A (en) * 1986-10-31 1991-02-05 Euroceltique, S.A. Controlled release hydromorphone composition
US4832967A (en) * 1986-11-17 1989-05-23 Rhone-Poulenc Sante Composition for feeding ruminants containing a biologically active substance and its preparation
US4842863A (en) * 1987-01-26 1989-06-27 Showa Denko Kabushiki Kaisha Granular agent for ruminant and production method thereof
US5064650A (en) * 1988-04-19 1991-11-12 Southwest Research Institute Controlled-release salt sensitive capsule for oral use and adhesive system
US5164195A (en) * 1988-04-19 1992-11-17 Southwest Research Institute Method of oral delivery with an adherent controlled-release salt sensitive capsule
US4880646A (en) * 1988-11-29 1989-11-14 Southwest Research Institute Encapsulated corn kernels and method of forming the same
US5132125A (en) * 1988-11-29 1992-07-21 Southwest Research Institute Encapsulated corn kernels and method of forming the same
US4971804A (en) * 1989-02-02 1990-11-20 Warner-Lambert Company Water dispersible gemfibrozil compositions
US5093128A (en) * 1989-07-18 1992-03-03 Draguesku Oliver J Rumen and other stomach chamber bypass nutrients and methods of fabrication
US5167947A (en) * 1989-10-26 1992-12-01 Southwest Research Institute Enhancement of absorption of radioprotective drugs
US5167962A (en) * 1990-05-23 1992-12-01 Southwest Research Institute Filament system for delivering a medicament and method
US5043169A (en) * 1990-05-25 1991-08-27 Warner-Lambert Company Stabilized Sweetner Composition
US5246636A (en) * 1991-05-07 1993-09-21 Southwest Research Institute Process for making microcapsules and apparatus therefor
US5190775A (en) * 1991-05-29 1993-03-02 Balchem Corporation Encapsulated bioactive substances
US5254598A (en) 1991-12-09 1993-10-19 Southwest Research Institute Biodegradable composition and products

Non-Patent Citations (16)

* Cited by examiner, † Cited by third party
Title
"Variety of Food Applications".
Dow Chemical, "Methocel Premium Food Gums".
Dow Chemical, "Thermal Gelation In Methocel Food Gums".
Dow Chemical, Methocel Premium Food Gums . *
Dow Chemical, Thermal Gelation In Methocel Food Gums . *
Food Engineering, Ingredients Vegetable oil encapsulates salt to overcome functional problems, May 1978, p. 57. *
Food Engineering, Ingredients--Vegetable oil encapsulates salt to overcome functional problems, May 1978, p. 57.
Graves, R.E., Cereal Science Today, Apr. 1972, vol. 17, No. 4, pp. 107 109. *
Graves, R.E., Cereal Science Today, Apr. 1972, vol. 17, No. 4, pp. 107-109.
J.M. Huber Corporation, "A New Synthetic Calcium Silicate for a Wide, 1987".
J.M. Huber Corporation, A New Synthetic Calcium Silicate for a Wide, 1987 . *
Southwest Research Institute, "A Capability Statement for Microencapsulation".
Southwest Research Institute, "Microencapsulation".
Southwest Research Institute, A Capability Statement for Microencapsulation . *
Southwest Research Institute, Microencapsulation . *
Variety of Food Applications . *

Cited By (51)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6610348B2 (en) 1997-02-17 2003-08-26 Fonterra Tech Limited Gelling agents and gels containing them
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US20020187221A1 (en) * 2001-04-26 2002-12-12 Takasago International Corporation Coating agent and coated powder
US20030124228A1 (en) * 2001-04-26 2003-07-03 Takasago International Corporation Coating agent and coated powder
US20040156953A1 (en) * 2003-02-12 2004-08-12 Guidry Ray A. Encapsulated food additives and method for preparing foodstuffs
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US20070031582A1 (en) * 2003-04-08 2007-02-08 Jack Burger Oxigen stable active containing compositions
US20060124695A1 (en) * 2003-06-27 2006-06-15 Wakunaga Pharmaceutical Co., Ltd. Stable liquid preparation
US20080317681A1 (en) * 2003-07-11 2008-12-25 Petros Gebreselassie Compositions containing a stain removing complex, and methods of making and using the same
US20070071808A1 (en) * 2003-08-28 2007-03-29 Janik John J Capsule filled with honey
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US20050260266A1 (en) * 2003-11-21 2005-11-24 Cadbury Adams Usa, Llc. Controlled release oral delivery systems
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US20070053972A1 (en) * 2005-09-08 2007-03-08 Cadbury Adams Usa Llc. Gelatin capsules containing actives
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US20080029110A1 (en) * 2006-02-10 2008-02-07 R. J. Reynolds Tobacco Company Smokeless Tobacco Composition
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US20110061666A1 (en) * 2006-02-10 2011-03-17 R. J. Reynolds Tobacco Company Smokeless Tobacco Composition
US20110097449A1 (en) * 2006-06-30 2011-04-28 Conagra Foods Rdm, Inc. Seasoning and method for seasoning a food product while reducing dietary sodium intake
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